A kind of heavy metal absorbent and its preparation
Technical field
The invention belongs to the absorption of heavy metal ion and stabilization technique, more particularly, to a kind of heavy metal absorbent and its system
It is standby.
Background technology
In recent years, heavy metal pollution event in China's takes place frequently.Heavy metal element chemical property is stable, along with the quick of industry
Development and the quickening of urbanization process, the heavy metal pollution in China is increasingly severe, substantial amounts of heavy metal be discharged into soil and river,
In lake and ocean, and by number of ways such as water, gas, solid wastes, long term accumulation, food chain are enriched with step by step in the environment, are finally entered
Enter human body accumulation so that the content of beary metal for staying in human body amplifies at double, to economic development, to ecological environment, food security and
Health constitutes a serious threat.
The exploitation of high-activity nano environmental purifying agent and production technology is the important support of environmental protection industry sustainable development.Receive
Rice magnesia has that specific surface area is big, surface-active is high, and heavy metal ion has very strong adsorption capacity, meanwhile, it is nano oxidized
There is magnesium surface the defects of magnesium room and Lacking oxygen potential energy to adsorb some metals formation elementide, and metal is inhaled with defective bit
Attached effect is very strong, it might even be possible to changes the chemical property of metal cluster, is presented in Heavy Metal Pollution Control and field of environment protection
Go out unique advantage and application prospect.Graphene as a kind of New Two Dimensional carbon material, have specific surface area is big, absorption property is strong,
The advantages that radiation resistance is good, good application prospect is presented in terms of traditional adsorbent is substituted.
The content of the invention
It is an object of the invention to provide a kind of heavy metal absorbent and its preparation, solves the problems, such as that prior art is present.
A kind of heavy metal absorbent, including by graphene and the compound of nano magnesia composite synthesis, the graphene
Percentage by weight be 0.1%~10%, the particle diameter of the nano magnesia is 10nm~100nm.
A kind of preparation of heavy metal absorbent, is mainly included the following steps that:
S1. chemical oxidization method prepares graphite oxide;
S2. the step S1 graphite oxides prepared are placed in ultrasonic 2h in ultrasonic cleaning machine, obtain graphene oxide solution, to
Sodium borohydride solution is added in graphene oxide solution, sequentially adds soluble magnesium salting liquid, citric acid solution stirring;
S3. solution is heated to 80 DEG C under agitation, solution first becomes colloidal sol after 2-3h, continues to become solidifying after stirring 1-2h
Glue;
S4. step S3 is obtained into gel to be put into Muffle furnace, foam 2h at 150 DEG C;Then 450-600 in air atmosphere
DEG C calcining 1-3h.
Further, the mol ratio of citric acid and soluble magnesium salt is 1 in step S2:1.
Further, chemical oxidization method described in step S1 prepares graphite oxide and mainly included the following steps that:
S11. under the conditions of ice-water bath, the concentrated sulfuric acid is added into container, magnetic agitation, after temperature is reduced to below 4 DEG C,
Crystalline graphite powder is added, and is quickly stirred to being uniformly dispersed;
S12. sodium nitrate is added, potassium permanganate is slow added into the case of being kept stirring for, controlling reaction temperature does not surpass
4 DEG C are crossed, stirs 2h;
S13. mixture temperature is risen into 35 DEG C again to react 30 minutes, is then slowly added into distilled water, control temperature is 60
DEG C, solution is changed into yellowish-brown;
S14. 30% (v/v%) hydrogen peroxide is added after stirring reaction 1h until mixture becomes glassy yellow;
S15. and then washed repeatedly with the mixed liquor and hydrochloric acid of dilute sulfuric acid and hydrogen peroxide, be finally several with distillation water washing
Secondary, it is 7 to make pH, and obtained tan precipitate is fully dried in 50 DEG C of vacuum drying chamber.
Further, graphite oxide described in step S2:Sodium borohydride:Soluble magnesium salt:The mass ratio of citric acid is 1:
1-4:50-1000:50-1000。
Further, the crystalline graphite powder, sodium nitrate, potassium permanganate, sulfuric acid mass ratio are 2:1-3:3-6:50-80.
Compared with prior art, the present invention includes the compound by graphene and nano magnesia composite synthesis, wherein oxygen
Changing magnesium heavy metal has strong absorption property, and graphene is the conductive 2D materials of unique texture, and there is excellent electronics to shift
Performance, and nano magnesia it is compound after can improve the absorption property of heavy metal.Both interactions, it will be advantageous to nano oxygen
Change growing, disperseing for magnesium, improve its conductive capability, promote the transmission of electronics, and then improve its performance.Therefore the present invention is due to tool
Have that specific surface area is big, unique absorption advantage of 2D materials, the removal of heavy metal ion has that adsorption capacity is big, processing time
Short, the advantages that treatment effeciency is high, the processing to heavy metal ions in wastewater has remarkable result.And the present invention is coagulated using colloidal sol
Prepared by glue method is well mixed, and simple for process, suitable for industrialized production, obtained particle diameter is small, is evenly distributed, and compares surface
Product is big.
Embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention will be made below further detailed
Description.
Embodiment 1
A kind of preparation of heavy metal absorbent, is mainly included the following steps that:
(1) using chemistry redox method synthesis graphite oxide:Under the conditions of ice-water bath, added into glass round bottom flask
The 50ml concentrated sulfuric acid (98%), magnetic agitation, after temperature is reduced to below 4 DEG C, adds 2.0g crystalline graphite powder, and quickly
Stirring the rear sodium nitrate for adding 1.0g, is slow added into 5.0g potassium permanganate, controlled to being uniformly dispersed in the case of being kept stirring for
Reaction temperature processed is no more than 4 DEG C, stirs 2h.Mixture temperature is risen into 35 DEG C again to react 30 minutes, is then slowly added into 100ml
Distilled water, control temperature at 60 DEG C, solution is changed into yellowish-brown, adds a certain amount of 30% (v/v%'s) after stirring reaction 1h
Hydrogen peroxide becomes glassy yellow until mixture.Then washed repeatedly with dilute sulfuric acid (5wt.%)+dioxygen water mixed liquid and hydrochloric acid,
Water washing with distillation several times, making its pH~7 finally, obtained tan precipitate is fully dried in 50 DEG C of vacuum drying chamber,
Obtain product graphite oxide 1.6g.
(2) sol-gal process prepares nano magnesia, graphene predecessor.Graphite oxide made from step (1) will be taken to take
0.1g is scattered in 30ml water, is ultrasonically treated 2h, obtains the graphene oxide suspension of brown, adds 250ml water, and dilution obtains
280ml graphene oxide suspensions, are kept stirring for.
(3) 0.2g sodium borohydrides are weighed, are dissolved in 20ml distilled water, are quickly poured into step (2) graphene oxide suspension
In, partial reduction graphene solution is obtained, continues to stir.
(4) 63.0g magnesium nitrate hexahydrates are weighed, adds in partial reduction graphene suspension obtained by step (3), keeps stirring
Mix until magnesium nitrate hexahydrate is completely dissolved.
(5) 36.0g citric acids (CA) are weighed and are dissolved in 100mL water, is added in step (3) resulting solution, is warming up to 80 DEG C of perseverances
Tepidarium, 4h is stirred, obtains wet gel.
(6) wet gel is put into 150 DEG C of degree drying boxes the 2h that foams, obtains xerogel.
(7) xerogel obtained by step (6) is put into after 2 DEG C/min is warming up to 450 DEG C in Muffle furnace and is incubated 2h.
Obtain the nano magnesia graphene Compound Heavy Metals adsorbent that graphene content is 1%, the adsorbent pair
Pb in 200ppm lead waste water2+Adsorption capacity be 1316mg/g.
Embodiment 2
A kind of preparation of heavy metal absorbent, is mainly included the following steps that:
(1) using chemistry redox method synthesis graphite oxide:Under the conditions of ice-water bath, added into glass round bottom flask
The 50ml concentrated sulfuric acid (98%), magnetic agitation, after temperature is reduced to below 4 DEG C, adds 2.0g crystalline graphite powder, and quickly
Stirring the rear sodium nitrate for adding 1.0g, is slow added into 5.0g potassium permanganate, controlled to being uniformly dispersed in the case of being kept stirring for
Reaction temperature processed is no more than 4 DEG C, stirs 2h.Mixture temperature is risen into 35 DEG C again to react 30 minutes, is then slowly added into 100ml
Distilled water, control temperature at 60 DEG C, solution is changed into yellowish-brown, adds a certain amount of 30% (v/v%'s) after stirring reaction 1h
Hydrogen peroxide becomes glassy yellow until mixture.Then washed repeatedly with dilute sulfuric acid (5wt%)+dioxygen water mixed liquid and hydrochloric acid,
Water washing with distillation several times, making its pH~7 finally, obtained tan precipitate is fully dried in 50 DEG C of vacuum drying chamber,
Obtain product graphite oxide 1.6g.
(2) sol-gal process prepares nano magnesia, graphene predecessor.Graphite oxide made from step (1) will be taken to take
1.0g is scattered in 30ml water, is ultrasonically treated 2h, obtains the graphene oxide suspension of brown, adds 250ml water, and dilution obtains
280ml graphene oxide suspensions, are kept stirring for.
(3) 0.2g sodium borohydrides are weighed, are dissolved in 20ml distilled water, are quickly poured into step (2) graphene oxide suspension
In, partial reduction graphene solution is obtained, continues to stir.
(4) 57.3g magnesium nitrate hexahydrates are weighed, adds in partial reduction graphene suspension obtained by step (3), keeps stirring
Mix until magnesium nitrate hexahydrate is completely dissolved.
(5) 32.0g citric acids are weighed and are dissolved in 100mL water, is added in step (3) resulting solution, is warming up to 80 DEG C of thermostatted waters
Bath, 4h is stirred, obtains wet gel.
(6) wet gel is put into 150 DEG C of degree drying boxes the 2h that foams, obtains xerogel.
(7) xerogel obtained by step (6) is put into after 2 DEG C/min is warming up to 600 DEG C in Muffle furnace and is incubated 2h.
Obtain the nano magnesia graphene Compound Heavy Metals adsorbent that graphene content is 10%, the adsorbent pair
Pb in 200ppm lead waste water2+Adsorption capacity be 1662mg/g.
Embodiment proposed by the present invention, as it will be easily appreciated by one skilled in the art that the above example table that applicant proposes
Bright technical solution of the invention is feasible.Simply embodiment described above is only presently preferred embodiments of the present invention, not
The present invention can be limited with this.All any modifications made within technical solution proposed by the present invention, equivalent substitution and change
Enter, should be included in the scope of the protection.